CN109056309B - Flexible electrode material and preparation method thereof - Google Patents

Flexible electrode material and preparation method thereof Download PDF

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Publication number
CN109056309B
CN109056309B CN201810907335.XA CN201810907335A CN109056309B CN 109056309 B CN109056309 B CN 109056309B CN 201810907335 A CN201810907335 A CN 201810907335A CN 109056309 B CN109056309 B CN 109056309B
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fabric
electrode material
flexible electrode
aqueous solution
titanium dioxide
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CN109056309A (en
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冯栋
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Daqing Haina Technology Co.,Ltd.
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Suzhou Hanxuan Information Technology Co ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • D06M11/65—Salts of oxyacids of nitrogen
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • D06M13/295—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof containing polyglycol moieties; containing neopentyl moieties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46—Compounds containing quaternary nitrogen atoms
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53—Polyethers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/10—Animal fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
    • D06M2101/28—Acrylonitrile; Methacrylonitrile
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50—Modified hand or grip properties; Softening compositions

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a preparation method of a flexible electrode material, which comprises the following steps: activating the fabric in a nitric acid aqueous solution at 80-95 ℃ for 1-2h according to the mass ratio of 1:10-20 to obtain an activated fabric; soaking the activated fabric in an aqueous solution of titanyl sulfate according to the mass ratio of 1:5-10, wherein the concentration of the aqueous solution of titanyl sulfate is 3-8mmol/L, then adding urea serving as a precipitating agent into the aqueous solution, and reacting at the temperature of 120-140 ℃ to obtain the fabric deposited with titanium dioxide; immersing the fabric deposited with the titanium dioxide into the carbon nano tube dispersion liquid, and treating at 80-110 ℃ to obtain a flexible electrode material; wherein, the carbon nano tube dispersion liquid comprises carbon nano tubes, a cationic surfactant containing nitrogen and/or phosphorus elements and water. The flexible electrode material prepared by the invention has the characteristics of air permeability, flexibility and stretchability of fabric, and also has antibacterial performance and good electrochemical performance.

Description

Flexible electrode material and preparation method thereof
Technical Field
The invention relates to the technical field of electrode materials, in particular to a flexible electrode material and a preparation method thereof.
Background
The wearable electronic product can be obtained by implanting electronic elements into the fabric, so that the garment has more electronic information functions on the basis of keeping comfort. The wearable electronic product has good application prospect in the aspects of continuous personal health monitoring devices, high-performance sports wear, flexible displays and the like. However, electronic products all require power supply, and thus energy conversion or storage equipment having properties of light weight, flexibility, breathability, and stretchability, which are unique to textiles, is necessary.
The carbon material has high specific surface area, good conductivity and stable chemical performance. Carbon nanotubes have a large aspect ratio and a hollow structure, so that they have a large specific surface area in order to store a large amount of charges. In addition, the carbon nano tube also has good conductivity and chemical stability, and can provide larger cycle stability and service life when preparing the energy storage material.
In the technology of using carbon nanotubes to treat fabric as electrode material, there are certain disadvantages, such as less carbon nanotube adsorption and not significantly improved conductivity, and the addition of crosslinking agent or adhesive to increase the adsorption of carbon nanotubes on fabric can seriously affect the fabric hand feeling.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a flexible electrode material and a preparation method thereof.
In one aspect, the present invention provides a method for preparing a flexible electrode material, comprising the steps of:
the preparation method of the flexible electrode material is characterized by comprising the following steps of:
(1) activating the fabric in a nitric acid aqueous solution at 80-95 ℃ for 1-2h according to the mass ratio of 1:10-20 to obtain an activated fabric;
(2) soaking the activated fabric in an aqueous solution of titanyl sulfate according to the mass ratio of 1:5-10, wherein the concentration of the aqueous solution of titanyl sulfate is 3mmol/L-8mmol/L, then adding urea as a precipitator into the aqueous solution, and reacting at the temperature of 120-140 ℃ to obtain the fabric deposited with titanium dioxide;
(3) immersing the fabric deposited with the titanium dioxide into a carbon nano tube dispersion liquid, and treating for 1-2h at 80-110 ℃ to obtain the flexible electrode material; wherein the carbon nanotube dispersion liquid comprises carbon nanotubes, a cationic surfactant containing nitrogen and/or phosphorus elements and water.
Further, in the step (1), the mass concentration of the nitric acid aqueous solution is 0.1 wt% to 1 wt%.
Further, in the step (1), the fabric is made of one or more of cotton, hemp, silk, terylene and acrylon.
Further, in the step (2), the molar ratio of the urea to the titanyl sulfate is 1-10: 1.
Further, in the step (2), the reaction time is 2-4 h.
Further, in the step (3), the mass fraction of the carbon nanotubes in the carbon nanotube dispersion is 5 to 20%, and the mass ratio of the fabric deposited with the titanium dioxide to the carbon nanotubes is 1:0.1 to 0.25.
Further, in the step (3), the cationic surfactant is one or more of fatty amine, polyoxyethylene fatty amine, quaternary ammonium salt, polyoxyethylene quaternary ammonium salt and polyoxyethylene ether phosphate.
Further, in the step (3), the mass ratio of the cationic surfactant to the carbon nanotubes is 0.01-0.05: 1.
Further, in the step (3), the particle size of the carbon nanotube is 10 to 50 nm.
In the step (1), the fabric is activated in nitric acid, so that the number of reactive groups and the hydrophilicity of the fabric can be enhanced, and the subsequent adsorption of carbon nanotubes on the surface of the fabric is facilitated. In addition, in the subsequent step, the cationic surfactant containing nitrogen and/or phosphorus elements in the carbon nanotube dispersion liquid is used, so that the dispersibility of the carbon nanotubes can be improved, the carbon nanotubes can be uniformly grafted to the surface of the fabric, and meanwhile, the N, P elements can also endow the fabric with flame retardant property.
In the step (2), the nano titanium dioxide is prepared by adopting a uniform precipitation method, so that the crystal-forming ions in the solution can be slowly and uniformly released from the solution, the added urea precipitator does not immediately react with the precipitation component, but slowly generates the nano particles through a chemical reaction, so that the generation speed of the nano particles is controlled, uniform and compact titanium dioxide nano particles are prepared, the particle size of the obtained nano particles is 30-80 nm, the requirement of the reaction on equipment is not high, and the preparation technology is simple.
In another aspect, the invention also claims a flexible electrode material prepared by the preparation method, which comprises a fabric, and titanium dioxide nano particles and carbon nano tubes connected with the fabric through coordination bonds.
The flexible electrode material prepared by the method has the specific capacitance value of 300F/g-500F/g and the air permeability of 10000g/m under the current density of 1A/g2/24h-20000g/m224 h; the electric conductivity reaches 120S/m to 180S/m, and the flame retardant property reaches more than four levels.
By the scheme, the invention at least has the following advantages:
according to the invention, a layer of titanium dioxide nano particles is deposited on the surface of the fabric, and the nano titanium dioxide has the characteristics of antibacterial property, excellent high rate performance and cycling stability, rapid charge and discharge performance and higher capacity, and high photoelectric conversion rate, so that the energy conversion rate of the electrode can be greatly improved by introducing the titanium dioxide nano particles into the flexible electrode material. And then forming a layer of carbon nanotube film on the surface of the fabric sample modified by the nano titanium dioxide, thereby preparing the flexible electrode material which has good conductivity, softness and stretchability of the fabric and good flame retardant effect. The preparation method of the flexible electrode provided by the scheme is simple, novel, green, environment-friendly, safe and efficient.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a preferred embodiment of the present invention and is described in detail below.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment provides a flexible electrode material and a preparation method thereof, and the preparation method comprises the following specific steps:
adding the pure cotton fabric into 0.8 wt% nitric acid water solution according to the mass ratio of 1:10, activating for 1h at 90 ℃, taking out the activated cotton fabric, and drying. Then soaking the dried fabric in a 3mmol/L titanyl sulfate aqueous solution for 15min according to the mass ratio of 1: 10; then adding urea into the mixture, wherein the molar ratio of the urea to the titanyl sulfate is 1:1, reacting for 2 hours at 120 ℃, taking out the reacted fabric, and washing the fabric to be neutral to obtain the fabric deposited with titanium dioxide.
Immersing the fabric deposited with the titanium dioxide into the dispersion liquid, and treating for 1h at 80 ℃ to obtain a flexible electrode material; wherein the carbon nanotube dispersion liquid comprises carbon nanotubes (the particle diameter is 10-15nm), a cationic surfactant containing nitrogen and/or phosphorus elements and water. Specifically, the mass fraction of carbon nanotubes in the carbon nanotube dispersion was 5%, and the mass ratio of the mass of the fabric deposited with titanium dioxide to the mass of carbon nanotubes was 1: 0.1. The mass ratio of the cationic surfactant to the carbon nanotubes was 0.01: 1. The cationic surfactant is one or more of fatty amine, polyoxyethylene fatty amine, quaternary ammonium salt, polyoxyethylene quaternary ammonium salt and polyoxyethylene ether phosphate.
The obtained flexible electrode material is cut into a size of 3cm multiplied by 2cm, and electrochemical test is carried out on an RST electrochemical workstation. Wherein the electrolyte is 0.5M KCl solution, the auxiliary electrode is a Pt electrode, the reference electrode is an Ag/AgCl electrode, the working electrode is a flexible electrode prepared by the method, and a three-electrode system is adopted for electrochemical test. The specific capacitance value of the flexible electrode material reaches 400F/g and the air permeability reaches 15000g/m under the current density of 1A/g224h, the electric conductivity reaches 120S/m, and the flame retardant performance reaches four levelsThe above.
Example 2
The embodiment provides a flexible electrode material and a preparation method thereof, and the preparation method comprises the following specific steps:
adding the silk fabric into 1wt% nitric acid water solution according to the mass ratio of 1:15, activating for 1h at 80 ℃, taking out the activated silk fabric, and drying. Then soaking the dried fabric in an aqueous solution of 8mmol/L titanyl sulfate for 15min according to the mass ratio of 1: 8; then adding urea into the mixture, wherein the molar ratio of the urea to the titanyl sulfate is 5:1, reacting for 2 hours at 140 ℃, taking out the reacted fabric, and washing the fabric to be neutral to obtain the fabric deposited with titanium dioxide.
Immersing the fabric deposited with the titanium dioxide into the dispersion liquid, and treating for 1h at 90 ℃ to obtain a flexible electrode material; wherein the carbon nanotube dispersion liquid comprises carbon nanotubes (the particle diameter is 15-20nm), a cationic surfactant containing nitrogen and/or phosphorus elements and water. Specifically, the mass fraction of carbon nanotubes in the carbon nanotube dispersion was 10%, and the mass ratio of the mass of the fabric deposited with titanium dioxide to the mass of carbon nanotubes was 1: 0.15. The mass ratio of the cationic surfactant to the carbon nanotubes was 0.03: 1. The cationic surfactant is one or more of fatty amine, polyoxyethylene fatty amine, quaternary ammonium salt, polyoxyethylene quaternary ammonium salt and polyoxyethylene ether phosphate.
The obtained flexible electrode material is cut into a size of 3cm multiplied by 2cm, and electrochemical test is carried out on an RST electrochemical workstation. Wherein the electrolyte is 0.5M KCl solution, the auxiliary electrode is a Pt electrode, the reference electrode is an Ag/AgCl electrode, the working electrode is a flexible electrode prepared by the method, and a three-electrode system is adopted for electrochemical test. The specific capacitance value of the flexible electrode material reaches 500F/g and the air permeability reaches 20000g/m under the current density of 1A/g2And 24h, the electric conductivity reaches 130S/m, and the flame retardant property reaches more than four levels.
Example 3
The embodiment provides a flexible electrode material and a preparation method thereof, and the preparation method comprises the following specific steps:
adding the ramie fabric into 0.5 wt% of nitric acid aqueous solution according to the mass ratio of 1:20, activating for 1h at 95 ℃, taking out the activated ramie fabric, and drying. Then soaking the dried fabric in 6mmol/L titanyl sulfate aqueous solution for 30min according to the mass ratio of 1: 10; then adding urea into the mixture, wherein the molar ratio of the urea to the titanyl sulfate is 10:1, reacting for 4 hours at 130 ℃, taking out the reacted fabric, and washing the fabric to be neutral to obtain the fabric deposited with titanium dioxide.
Immersing the fabric deposited with the titanium dioxide into the dispersion liquid, and treating for 2h at 100 ℃ to obtain a flexible electrode material; wherein the carbon nanotube dispersion liquid comprises carbon nanotubes (the particle diameter is 20-30nm), a cationic surfactant containing nitrogen and/or phosphorus elements and water. Specifically, the mass fraction of carbon nanotubes in the carbon nanotube dispersion was 15%, and the mass ratio of the mass of the fabric deposited with titanium dioxide to the mass of carbon nanotubes was 1: 0.2. The mass ratio of the cationic surfactant to the carbon nanotubes was 0.05: 1. The cationic surfactant is one or more of fatty amine, polyoxyethylene fatty amine, quaternary ammonium salt, polyoxyethylene quaternary ammonium salt and polyoxyethylene ether phosphate.
The obtained flexible electrode material is cut into a size of 3cm multiplied by 2cm, and electrochemical test is carried out on an RST electrochemical workstation. Wherein the electrolyte is 0.5M KCl solution, the auxiliary electrode is a Pt electrode, the reference electrode is an Ag/AgCl electrode, the working electrode is a flexible electrode prepared by the method, and a three-electrode system is adopted for electrochemical test. Under the current density of 1A/g, the specific capacitance value of the flexible electrode material reaches 460F/g, and the air permeability reaches 17000g/m2And 24h, the electric conductivity reaches 130S/m, and the flame retardant property reaches more than four levels.
Example 4
The embodiment provides a flexible electrode material and a preparation method thereof, and the preparation method comprises the following specific steps:
adding the silk fabric into 0.1 wt% nitric acid water solution according to the mass ratio of 1:10, activating for 2 hours at 95 ℃, taking out the activated silk fabric, and drying. Then soaking the dried fabric in a 7mmol/L titanyl sulfate aqueous solution for 30min according to the mass ratio of 1: 8; then adding urea into the mixture, wherein the molar ratio of the urea to the titanyl sulfate is 6:1, reacting for 3.5 hours at 135 ℃, taking out the reacted fabric, and washing the fabric to be neutral to obtain the fabric deposited with titanium dioxide.
Immersing the fabric deposited with the titanium dioxide into the dispersion liquid, and treating for 1.5h at 110 ℃ to obtain a flexible electrode material; wherein the carbon nanotube dispersion liquid comprises carbon nanotubes (the particle diameter is 30-40nm), a cationic surfactant containing nitrogen and/or phosphorus elements and water. Specifically, the mass fraction of carbon nanotubes in the carbon nanotube dispersion was 20%, and the mass ratio of the fabric deposited with titanium dioxide to the carbon nanotubes was 1: 0.25. The mass ratio of the cationic surfactant to the carbon nanotubes was 0.04: 1. The cationic surfactant is one or more of fatty amine, polyoxyethylene fatty amine, quaternary ammonium salt, polyoxyethylene quaternary ammonium salt and polyoxyethylene ether phosphate.
The obtained flexible electrode material is cut into a size of 3cm multiplied by 2cm, and electrochemical test is carried out on an RST electrochemical workstation. Wherein the electrolyte is 0.5M KCl solution, the auxiliary electrode is a Pt electrode, the reference electrode is an Ag/AgCl electrode, the working electrode is a flexible electrode prepared by the method, and a three-electrode system is adopted for electrochemical test. The specific capacitance value of the flexible electrode material reaches 400F/g and the air permeability reaches 17000g/m under the current density of 1A/g2And the electric conductivity reaches 180S/m after 24h, and the flame retardant property reaches more than four levels.
Example 5
The embodiment provides a flexible electrode material and a preparation method thereof, and the preparation method comprises the following specific steps:
prepared according to the method of example 4 with the difference that: the particle diameter of the carbon nano tube is 40-50nm), and the mass ratio of the fabric deposited with the titanium dioxide to the carbon nano tube is 1: 0.15. The mass ratio of the cationic surfactant to the carbon nanotubes was 0.02: 1. The cationic surfactant is one or more of fatty amine, polyoxyethylene fatty amine, quaternary ammonium salt, polyoxyethylene quaternary ammonium salt and polyoxyethylene ether phosphate.
The specific capacitance value of the flexible electrode material reaches 500F/g and the air permeability reaches 10000g/m under the current density of 1A/g2And the electric conductivity reaches 120S/m after 24h, and the flame retardant property reaches more than four levels.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (5)

1. The preparation method of the flexible electrode material is characterized by comprising the following steps of:
(1) activating the fabric in a nitric acid aqueous solution at 80-95 ℃ for 1-2h according to the mass ratio of 1:10-20 to obtain an activated fabric; the mass concentration of the nitric acid aqueous solution is 0.1-1 wt%;
(2) soaking the activated fabric in a titanyl sulfate aqueous solution according to the mass ratio of 1:5-10, wherein the concentration of the titanyl sulfate aqueous solution is 3mmol/L-8mmol/L, then adding urea serving as a precipitator into the titanyl sulfate aqueous solution, and reacting at the temperature of 120-140 ℃ to obtain the fabric deposited with titanium dioxide; the molar ratio of the urea to the titanyl sulfate is 1-10: 1;
(3) immersing the fabric deposited with the titanium dioxide into a carbon nano tube dispersion liquid, and treating for 1-2h at 80-110 ℃ to obtain the flexible electrode material; wherein the carbon nanotube dispersion liquid comprises carbon nanotubes, a cationic surfactant containing nitrogen and/or phosphorus elements and water; the mass fraction of the carbon nanotubes in the carbon nanotube dispersion liquid is 5-20%, and the mass ratio of the mass of the fabric deposited with the titanium dioxide to the mass of the carbon nanotubes is 1: 0.1-0.25; the particle size of the carbon nano tube is 10-50 nm; the cationic surfactant is one or more of fatty amine, quaternary ammonium salt and polyoxyethylene ether phosphate.
2. The method for preparing a flexible electrode material according to claim 1, wherein: in the step (1), the fabric is made of one or more of cotton, hemp, silk, terylene and acrylic fiber.
3. The method for preparing a flexible electrode material according to claim 1, wherein: in the step (2), the reaction time is 2-4 h.
4. The method for preparing a flexible electrode material according to claim 1, wherein: in the step (3), the mass ratio of the cationic surfactant to the carbon nanotubes is 0.01-0.05: 1.
5. A flexible electrode material prepared by the preparation method of any one of claims 1 to 4, which comprises a fabric, and titanium dioxide nanoparticles and carbon nanotubes connected with the fabric through coordination bonds.
CN201810907335.XA 2018-08-09 2018-08-09 Flexible electrode material and preparation method thereof Active CN109056309B (en)

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